HRID326845

反应详情

EQUATION

反应方程式

HRID 326845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

At about 50° C., 26.4 g (0.40 mole) of 85% potassium hydroxide are solubilized in 100 g (1.0 mole) of 2,2,2-trifluoroethanol. After cooling at 25° C., 37.8 g (0.50 mole) of chloroacetonitrile are added dropwise to this solution. The temperature rises slowly to 40° C. and a precipitate appears. The reaction mixture is then brought gradually to 60° C.; after the addition of 300 ml of heptane, it is then brought to reflux. The whole of the vapour is condensed by means of a Dean and Stark apparatus. The lower phase of the condensate is separated after settling has taken place and distilled at atmospheric pressure. Yld: 19.6 g (28%), b.p. 125°-140° C.

WORKUP

后处理

  1. customAt about 50° C.
  2. customrises slowly to 40° C.
  3. customis then brought gradually to 60° C.
  4. temperatureto reflux
  5. customcondensed by means of a Dean and Stark apparatus
  6. customThe lower phase of the condensate is separated after settling
  7. distillationdistilled at atmospheric pressure